JP2022045922A - Steel sheet - Google Patents
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- JP2022045922A JP2022045922A JP2021146269A JP2021146269A JP2022045922A JP 2022045922 A JP2022045922 A JP 2022045922A JP 2021146269 A JP2021146269 A JP 2021146269A JP 2021146269 A JP2021146269 A JP 2021146269A JP 2022045922 A JP2022045922 A JP 2022045922A
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- BNGXYYYYKUGPPF-UHFFFAOYSA-M (3-methylphenyl)methyl-triphenylphosphanium;chloride Chemical compound [Cl-].CC1=CC=CC(C[P+](C=2C=CC=CC=2)(C=2C=CC=CC=2)C=2C=CC=CC=2)=C1 BNGXYYYYKUGPPF-UHFFFAOYSA-M 0.000 description 1
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
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Abstract
Description
本発明は、せん断端面で発生する遅れ破壊を抑制可能とする鋼板に関する。 The present invention relates to a steel sheet capable of suppressing delayed fracture occurring at a shear end face.
近年、自動車の構造部材を軽量化する観点から、使用する鋼板を高強度化することによって板厚を低減する努力が進められている。このような鋼板の高強度化にともない、遅れ破壊が生じやすくなることが知られており、従来の自動車用部材では問題になることのなかった遅れ破壊に対する懸念が新たに浮上してきた。 In recent years, from the viewpoint of reducing the weight of structural members of automobiles, efforts have been made to reduce the thickness of the steel sheet used by increasing the strength. It is known that delayed fracture is likely to occur with the increase in strength of such steel sheets, and there is a new concern about delayed fracture, which has not been a problem with conventional automobile members.
遅れ破壊とは、高強度鋼部品が静的な負荷応力を受けた状態で、ある時間が経過したとき、外見的にはほとんど塑性変形を伴うことなしに、突然脆性的に破壊する現象である。広義には液体金属接触割れや応力腐食割れなども含まれるが、自動車用部品で問題になるのは腐食に伴い鋼中に侵入する水素によって引き起こされる水素脆化型の遅れ破壊である。遅れ破壊を引き起こす因子としては、材料（強度）、加工（歪・応力）、水素の３因子であることが知られている。ここで、金属材料への水素の侵入原因としては、金属材料と接触する溶液・溶媒からの侵入や、使用される環境下で金属材料が腐食することに伴って発生する水素の侵入が考えられる。 Delayed fracture is a phenomenon in which a high-strength steel part suddenly breaks brittlely after a certain period of time under static load stress, with almost no plastic deformation in appearance. .. In a broad sense, liquid metal contact cracking and stress corrosion cracking are also included, but the problem with automobile parts is the hydrogen embrittlement type delayed fracture caused by hydrogen that invades the steel due to corrosion. It is known that there are three factors that cause delayed fracture: material (strength), processing (strain / stress), and hydrogen. Here, the causes of hydrogen intrusion into the metal material are considered to be the intrusion from the solution / solvent that comes into contact with the metal material and the intrusion of hydrogen generated by the corrosion of the metal material in the environment in which it is used. ..
この遅れ破壊は、鋼板の場合についていえば、プレス成形により所定の形状に成形したときの残留引張り応力と、応力集中部における鋼の水素脆性により生じるものであることが知られている。 It is known that this delayed fracture is caused by the residual tensile stress when the steel sheet is formed into a predetermined shape by press forming and the hydrogen embrittlement of the steel in the stress concentration portion.
近年、１１８０ＭＰａ以上の高強度鋼板における遅れ破壊の評価方法についても、種々の提案がなされている。例えば、せん断加工後にＵ曲げ加工した試験片（鋼板）を用いて遅れ破壊特性を評価する方法が挙げられる。せん断加工後の鋼板のせん断端面には、ひずみ（刃と鋼板の接触による加工硬化や残留応力）およびひずみによる微小なき裂が生じる。このひずみおよび微小なき裂によって、Ｕ曲げ加工を施した鋼板のせん断端面の割れ発生頻度が異なることがあり、遅れ破壊特性におよぼすせん断端面の影響が問題となっている。また、実際の自動車用部材においてもせん断端面は存在するため、せん断端面のひずみおよび微小なき裂による遅れ破壊は大きな問題となりうる。 In recent years, various proposals have been made for evaluation methods for delayed fracture in high-strength steel plates of 1180 MPa or more. For example, there is a method of evaluating delayed fracture characteristics using a test piece (steel plate) that has been U-bent after shearing. Strain (work hardening and residual stress due to contact between the blade and the steel sheet) and minute cracks due to the strain occur on the sheared end face of the steel sheet after shearing. Due to this strain and minute cracks, the crack occurrence frequency of the sheared end face of the U-bented steel sheet may differ, and the influence of the sheared end face on the delayed fracture characteristics becomes a problem. Further, since the sheared end face also exists in an actual automobile member, the strain of the sheared end face and the delayed fracture due to a minute crack can be a big problem.
こうしたせん断端面の遅れ破壊特性を良くするため、特許文献１や特許文献２で開示された技術では、せん断条件または打ち抜き条件を制御することでせん断端面の残留応力を低下させている。
In order to improve such delayed fracture characteristics of the sheared end face, in the techniques disclosed in
しかしながら、これだけではせん断端面に発生する微小なき裂を抑制することが難しく、せん断端面の遅れ破壊を抑制することは難しい。さらに、せん断端面のみならず、せん断時に刃と鋼板が接触した部分については、刃と鋼板の接触による加工硬化や残留応力の影響を受ける。このため、刃と鋼板が接触する部分においても発生する微小なき裂を抑制する必要がある。 However, it is difficult to suppress minute cracks generated in the sheared end face by this alone, and it is difficult to suppress delayed fracture of the sheared end face. Further, not only the sheared end face but also the portion where the blade and the steel plate come into contact during shearing is affected by work hardening and residual stress due to the contact between the blade and the steel plate. Therefore, it is necessary to suppress minute cracks that occur even in the portion where the blade and the steel plate come into contact with each other.
本発明は、かかる事情に鑑みてなされたものであって、せん断時に刃と鋼板が接触する部分およびせん断端面の遅れ破壊を抑制可能な鋼板を提供することを目的とする。 The present invention has been made in view of such circumstances, and an object of the present invention is to provide a steel sheet capable of suppressing delayed fracture of a portion where a blade and a steel sheet come into contact with each other and a sheared end face during shearing.
本発明の要旨は次のとおりである。
［１］引張強さが１１８０ＭＰａ以上の鋼板であって、鋼板表面上に非金属からなる皮膜を有する鋼板の摩擦係数が０．５以下であり、前記皮膜の膜厚が１０ｎｍ以上であり、さらに、前記非金属からなる皮膜を有する鋼板の摩擦係数と前記皮膜の膜厚が式（１）を満たす鋼板。
（１／μ）×ｔ≧１００・・・（１）
なお、式（１）において、
μ：非金属からなる皮膜を有する鋼板の摩擦係数、ｔ：非金属からなる皮膜の膜厚（ｎｍ）
である。
［２］前記［１］に記載の鋼板において、鋼板表面上にめっき層を有し、前記めっき層上に前記非金属からなる皮膜を有する鋼板。
［３］前記［１］または［２］に記載の鋼板において、前記非金属からなる皮膜を有する鋼板の摩擦係数と前記皮膜の膜厚が式（２）を満たす鋼板。
（１／μ）×ｔ≧１０００・・・（２）
なお、式（２）において、
μ：非金属からなる皮膜を有する鋼板の摩擦係数、ｔ：非金属からなる皮膜の膜厚（ｎｍ）
である。
The gist of the present invention is as follows.
[1] A steel sheet having a tensile strength of 1180 MPa or more, having a steel sheet having a film made of a non-metal on the surface of the steel sheet, having a friction coefficient of 0.5 or less, the film having a film thickness of 10 nm or more, and further. , A steel sheet in which the friction coefficient of the steel sheet having a film made of the non-metal and the film thickness of the film satisfy the formula (1).
(1 / μ) × t ≧ 100 ... (1)
In addition, in equation (1)
μ: Friction coefficient of steel sheet having a film made of non-metal, t: Thickness of film made of non-metal (nm)
Is.
[2] In the steel sheet according to the above [1], a steel sheet having a plating layer on the surface of the steel sheet and having a film made of the non-metal on the plating layer.
[3] In the steel sheet according to the above [1] or [2], a steel sheet in which the friction coefficient of the steel sheet having a film made of the non-metal and the film thickness of the film satisfy the formula (2).
(1 / μ) × t ≧ 1000 ... (2)
In addition, in equation (2)
μ: Friction coefficient of steel sheet having a film made of non-metal, t: Thickness of film made of non-metal (nm)
Is.
本発明によれば、せん断時に刃と鋼板が接触する部分の微小なき裂や、せん断端面に入るひずみおよび微小なき裂の発生を抑制することができ、せん断端面の遅れ破壊特性を向上することが可能である。このため、本発明の鋼板は自動車用部材に好適である。 According to the present invention, it is possible to suppress the generation of minute cracks in the portion where the blade and the steel sheet come into contact during shearing, strains entering the sheared end face, and minute cracks, and it is possible to improve the delayed fracture characteristics of the sheared end face. It is possible. Therefore, the steel sheet of the present invention is suitable for automobile members.
本発明は、引張強さが１１８０ＭＰａ以上の鋼板であって、鋼板表面上に非金属からなる皮膜を有する鋼板の摩擦係数が０．５以下であって、皮膜の膜厚が１０ｎｍ以上であり、非金属からなる皮膜を有する鋼板の摩擦係数と膜厚が後述の式（１）を満たすことを特徴とする。 In the present invention, a steel sheet having a tensile strength of 1180 MPa or more, a steel sheet having a film made of a non-metal on the surface of the steel sheet has a coefficient of friction of 0.5 or less, and a film film thickness of 10 nm or more. It is characterized in that the coefficient of friction and the film thickness of the steel sheet having a film made of non-metal satisfy the formula (1) described later.
以下、本発明について説明する。 Hereinafter, the present invention will be described.
引張強さが１１８０ＭＰａ以上
本発明では、遅れ破壊が発生しやすい１１８０ＭＰａ以上の引張強さを有する鋼板を用いる。なお、鋼板表面上にはめっき層を有してもよい。鋼板の耐食性を向上させるため、鋼板表面にＺｎ、Ｆｅ、Ａｌ、Ｍｇ、Ｎｉ、およびＳｉを少なくとも１種類以上含むめっき層を有することが好ましい。また、めっき層を有する鋼板の場合、後述する非金属からなる皮膜は、めっき層上に形成されるものとする。
In the present invention, a steel sheet having a tensile strength of 1180 MPa or more, which is prone to delayed fracture, is used. A plating layer may be provided on the surface of the steel sheet. In order to improve the corrosion resistance of the steel sheet, it is preferable to have a plating layer containing at least one kind of Zn, Fe, Al, Mg, Ni, and Si on the surface of the steel sheet. Further, in the case of a steel plate having a plating layer, a film made of a non-metal described later is assumed to be formed on the plating layer.
鋼板表面に非金属からなる皮膜
せん断もしくは打ち抜きの刃が鋼板に直接あたると、せん断時に刃と鋼板が接触する部分およびせん断端面が押しつぶされて加工硬化してしまい、せん断時に刃と鋼板が接触する部分およびせん断端面には微小なき裂が入りやすくなる。この微小なき裂が遅れ破壊を起こしやすくするため、せん断もしくは打ち抜きの刃による加工硬化および微小なき裂の発生を抑える必要がある。なお、本発明において、せん断（機）の上刃および下刃、ならびに、打ち抜き（機）のポンチおよびダイスのことを、単に刃（可動刃）と称することもある。
A film made of non-metal on the surface of a steel plate When a sheared or punched blade directly hits a steel plate, the part where the blade and the steel plate contact during shearing and the sheared end face are crushed and hardened, and the blade and the steel plate come into contact during shearing. Small cracks are likely to enter the portion and the sheared end face. Since these minute cracks are prone to delayed fracture, it is necessary to suppress work hardening and the occurrence of minute cracks by shearing or punching blades. In the present invention, the upper and lower blades of the shear (machine) and the punches and dies of the punching (machine) may be simply referred to as blades (movable blades).
せん断端面のひずみによる加工硬化を抑制するため、本発明では鋼板表面上に非金属からなる皮膜を有する。皮膜が金属である場合、プレス成形の際に、皮膜が鋼板表面に凝着してしまう。このため、自動車用部材として化成処理や電着塗装をする際に、金属の凝着部が化成処理および電着塗装不良の原因となる。 In order to suppress work hardening due to strain on the sheared end face, the present invention has a film made of non-metal on the surface of the steel sheet. When the film is made of metal, the film adheres to the surface of the steel sheet during press molding. Therefore, when chemical conversion treatment or electrodeposition coating is performed as an automobile member, the metal adhesion portion causes chemical conversion treatment or electrodeposition coating failure.
鋼板表面上に非金属からなる皮膜を有することにより、せん断もしくは打ち抜きの刃と鋼板の間の摩擦係数を低下させる効果だけでなく、せん断もしくは打ち抜き時の圧縮応力を緩和させ、鋼板表面の加工硬化を抑制する効果がある。その結果、微小なき裂の発生を抑制し、せん断端面からの遅れ破壊を抑制可能とする。 Having a film made of non-metal on the surface of the steel sheet not only has the effect of lowering the friction coefficient between the shearing or punching blade and the steel sheet, but also alleviates the compressive stress during shearing or punching, and the surface of the steel sheet is processed and hardened. Has the effect of suppressing. As a result, it is possible to suppress the generation of minute cracks and suppress delayed fracture from the sheared end face.
非金属からなる皮膜を有する鋼板の摩擦係数が０．５以下
せん断端面のひずみ抑制効果を発現するためには、非金属からなる皮膜を有する鋼板の摩擦係数は、０．５以下とする。好ましくは０．３以下が望ましい。摩擦係数が小さくなると、鋼板とせん断もしくは打ち抜きの刃の間の面圧が小さくなり、ひずみが抑制しやすい。摩擦係数が０．５より大きいとひずみの抑制効果は発現できない。
The coefficient of friction of a steel sheet having a film made of non-metal is 0.5 or less. In order to exert the strain suppressing effect on the sheared end face, the coefficient of friction of the steel sheet having a film made of non-metal shall be 0.5 or less. It is preferably 0.3 or less. When the coefficient of friction becomes small, the surface pressure between the steel sheet and the shearing or punching blade becomes small, and strain is easily suppressed. If the coefficient of friction is larger than 0.5, the effect of suppressing strain cannot be exhibited.
皮膜の膜厚が１０ｎｍ以上
皮膜の膜厚は１０ｎｍ以上とする。皮膜の膜厚が１０ｎｍ未満であると、皮膜が薄いため、ひずみおよび微小なき裂の抑制効果は発現できない。さらに、皮膜によるクッション効果によるひずみ抑制を発現するためには皮膜の厚さは、好ましくは１００ｎｍ以上、より好ましくは１０００ｎｍ以上であることが望ましい。一方、皮膜の膜厚が大きくなると所定のプレス成形が難しくなることと、コスト高を招くことから皮膜の膜厚は１ｍｍ以下とすることが好ましい。
The film thickness is 10 nm or more. The film thickness is 10 nm or more. If the film thickness is less than 10 nm, the effect of suppressing strain and minute cracks cannot be exhibited because the film is thin. Further, in order to exhibit the strain suppression due to the cushioning effect of the film, the thickness of the film is preferably 100 nm or more, more preferably 1000 nm or more. On the other hand, when the film thickness of the film is large, it becomes difficult to perform a predetermined press molding, and the cost is high. Therefore, the film thickness is preferably 1 mm or less.
なお、皮膜の膜厚は、後述する実施例の方法により測定すればよい。 The film thickness may be measured by the method of Examples described later.
非金属からなる皮膜を有する鋼板の摩擦係数と膜厚が下記式（１）を満たす。
（１／μ）×ｔ≧１００・・・（１）
なお、式（１）において、
μ：非金属からなる皮膜を有する鋼板の摩擦係数、ｔ：非金属からなる皮膜の膜厚（ｎｍ）
である。
The coefficient of friction and the film thickness of the steel sheet having a film made of non-metal satisfy the following formula (1).
(1 / μ) × t ≧ 100 ... (1)
In addition, in equation (1)
μ: Friction coefficient of steel sheet having a film made of non-metal, t: Thickness of film made of non-metal (nm)
Is.
好ましくは、非金属からなる皮膜を有する鋼板の摩擦係数と皮膜の膜厚が下記式（２）を満たす。
（１／μ）×ｔ≧１０００・・・（２）
μ：非金属からなる皮膜を有する鋼板の摩擦係数、ｔ：非金属からなる皮膜の膜厚（ｎｍ）
である。
Preferably, the coefficient of friction of the steel sheet having a film made of a non-metal and the film thickness of the film satisfy the following formula (2).
(1 / μ) × t ≧ 1000 ... (2)
μ: Friction coefficient of steel sheet having a film made of non-metal, t: Thickness of film made of non-metal (nm)
Is.
皮膜には、せん断もしくは打ち抜きの刃と鋼板の間の摩擦係数を低下させる効果だけでなく、せん断もしくは打ち抜き時の圧縮応力を緩和させ、鋼板表面の加工硬化を抑制する効果がある。このため、式（１）の範囲外の場合は、摩擦係数が大きく、膜厚が薄い場合となり、ひずみおよび微小き裂抑制効果が小さい。 The film not only has the effect of reducing the coefficient of friction between the shearing or punching blade and the steel sheet, but also has the effect of relaxing the compressive stress during shearing or punching and suppressing work hardening of the steel sheet surface. Therefore, when it is out of the range of the equation (1), the friction coefficient is large and the film thickness is thin, and the strain and the effect of suppressing minute cracks are small.
本発明における皮膜の種類は、特段限定する必要はないが、例えば、無機系皮膜、有機系皮膜があげられる。無機系皮膜として、Ｍｎ－Ｐ系酸化物皮膜、Ｎｉ系無機皮膜、亜鉛系酸化皮膜、銅系酸化皮膜、鉄系酸化皮膜があげられる。また、有機系皮膜として、ポリ塩化ビニル系樹脂、ポリエチレン系樹脂、ポリプロピレン系樹脂、エポキシ樹脂、ポリヒドロキシポリエーテル樹脂、ポリエステル樹脂、ウレタン樹脂、シリコン樹脂、アクリル樹脂があげられる。また、皮膜は、有機無機複合皮膜であっても効果を発現することができる。 The type of film in the present invention is not particularly limited, and examples thereof include an inorganic film and an organic film. Examples of the inorganic film include a Mn—P-based oxide film, a Ni-based inorganic film, a zinc-based oxide film, a copper-based oxide film, and an iron-based oxide film. Examples of the organic film include a polyvinyl chloride resin, a polyethylene resin, a polypropylene resin, an epoxy resin, a polyhydroxypolyether resin, a polyester resin, a urethane resin, a silicon resin, and an acrylic resin. Further, even if the film is an organic-inorganic composite film, the effect can be exhibited.
次に、本発明の鋼板の製造方法について説明する。 Next, the method for manufacturing the steel sheet of the present invention will be described.
本発明の鋼板は、引張強さが１１８０ＭＰａ以上の鋼板に非金属からなる皮膜を付与することにより得ることができる。 The steel sheet of the present invention can be obtained by applying a film made of a non-metal to a steel sheet having a tensile strength of 1180 MPa or more.
鋼板表面に皮膜を付与する方法としては、前処理後に皮膜を付与すればよい。鋼板に所定の引張強さを確保するため、固溶強化元素のＳｉや、マルテンサイト変態を容易にするＭｎ等が軟鋼に比べて多く含まれる。このため、鋼板表面またはめっき層表面にはＳｉやＭｎなどの高温酸化物が形成する。この酸化物によって鋼板表面またはめっき層表面が不活性になり、無機系皮膜、有機系皮膜、有機無機複合皮膜を効果的に付与することが難しい。そこで、皮膜付与の前処理として、酸性の溶液に鋼板を浸漬し、ＳｉやＭｎなどの酸化物を除去する必要がある。酸性の溶液は特に限定しないが、好ましくは、ＳｉやＭｎを効果的に除去するため、フッ化水素酸（３０～５０％）／過酸化水素の液量比率が１／３０～１／９となるように混合し、液温度が１０～７０℃になるよう調整すればよい。この酸性溶液に鋼板を１～１０秒浸漬し、その後、飽和の炭酸水素ナトリウムに浸漬して表面を中和することで皮膜を効果的に付与可能となる。また、酸性溶液に浸漬してＳｉやＭｎなどの高温酸化物の除去が難しい場合は、鋼板表面に電気めっきによるＦｅめっきもしくはＺｎめっきを施してもよい。鋼板表面上の高温酸化物を電気めっき層で覆い、表面が活性になることで無機系皮膜、有機系皮膜、有機無機複合皮膜を効果的に付与可能となる。 As a method of applying a film to the surface of the steel sheet, a film may be applied after the pretreatment. In order to secure a predetermined tensile strength in the steel sheet, Si, which is a solid solution strengthening element, and Mn, which facilitates martensitic transformation, are contained in a larger amount than in mild steel. Therefore, high-temperature oxides such as Si and Mn are formed on the surface of the steel sheet or the surface of the plating layer. This oxide inactivates the surface of the steel sheet or the surface of the plating layer, and it is difficult to effectively apply an inorganic film, an organic film, or an organic-inorganic composite film. Therefore, as a pretreatment for applying the film, it is necessary to immerse the steel sheet in an acidic solution to remove oxides such as Si and Mn. The acidic solution is not particularly limited, but preferably, the hydrofluoric acid (30 to 50%) / hydrogen peroxide solution amount ratio is 1/30 to 1/9 in order to effectively remove Si and Mn. It may be adjusted so that the liquid temperature becomes 10 to 70 ° C. A film can be effectively applied by immersing the steel sheet in this acidic solution for 1 to 10 seconds and then immersing it in saturated sodium hydrogen carbonate to neutralize the surface. If it is difficult to remove high-temperature oxides such as Si and Mn by immersing in an acidic solution, the surface of the steel sheet may be subjected to Fe plating or Zn plating by electroplating. The high-temperature oxide on the surface of the steel sheet is covered with an electroplating layer, and the surface becomes active, so that an inorganic film, an organic film, and an organic-inorganic composite film can be effectively applied.
無機系皮膜、有機系皮膜、有機無機複合皮膜においては、皮膜成分を含む塗料を鋼板表面に塗布する手段は特に限定しないが、浸漬やロールコータが好適に用いられる。乾燥は、室温での自然乾燥または加熱乾燥による焼き付け処理が用いられる。加熱乾燥による焼き付け処理は、ドライヤー熱風炉、高周波誘導加熱炉、赤外線炉などを用いることができる。加熱乾燥による焼き付け処理は、到達板温で５０～３５０℃、好ましくは、８０～２５０℃の範囲が特に好ましい。加熱温度が５０℃未満では皮膜中の溶媒が多量に残り、耐食性が不十分となる。また、加熱温度が３５０℃を超えると非経済的であるばかりでなく、皮膜に欠陥が生じて耐食性が低下する恐れがある。 In the inorganic film, the organic film, and the organic-inorganic composite film, the means for applying the paint containing the film component to the surface of the steel sheet is not particularly limited, but dipping or a roll coater is preferably used. For drying, a baking process by natural drying at room temperature or heat drying is used. For the baking treatment by heating and drying, a dryer hot air furnace, a high frequency induction heating furnace, an infrared furnace, or the like can be used. The baking treatment by heat drying is particularly preferably in the range of 50 to 350 ° C., preferably 80 to 250 ° C. at the ultimate plate temperature. If the heating temperature is less than 50 ° C., a large amount of solvent remains in the film, resulting in insufficient corrosion resistance. Further, if the heating temperature exceeds 350 ° C., not only is it uneconomical, but also the film may be defective and the corrosion resistance may be deteriorated.
ここで、皮膜の膜厚については、浸漬の場合は浸漬時間を変える、ロールコータの場合はロールの圧下力やロールの回転速度、塗料の粘度を変えることにより制御すればよい。また、摩擦係数については、付与する皮膜の種類により定まるものである。 Here, the film thickness may be controlled by changing the immersion time in the case of immersion, or changing the rolling force, the rotation speed of the roll, and the viscosity of the paint in the case of a roll coater. The coefficient of friction is determined by the type of film to be applied.
本発明について実施例を用いて説明する。なお、本発明は以下の実施例に限定されない。 The present invention will be described with reference to examples. The present invention is not limited to the following examples.
皮膜の種類は、表１に示す通り、皮膜なし、有機系皮膜のエポキシ系樹脂、有機無機複合皮膜のエポキシ系樹脂／結晶性層状物、無機系皮膜の塩基性硫酸亜鉛３～５水和物とした。表１に示す各皮膜を、表２に示す１．４ｍｍ厚の冷延鋼板または各めっき鋼板表面上に設けた。 As shown in Table 1, the types of film are as shown in Table 1, no film, organic film epoxy resin, organic-inorganic composite film epoxy resin / crystalline layered material, and inorganic film basic zinc sulfate 3-5 hydrate. And said. Each film shown in Table 1 was provided on the surface of a 1.4 mm thick cold-rolled steel sheet or each plated steel sheet shown in Table 2.
皮膜形成に際し、冷延鋼板またはめっき鋼板をアルカリ脱脂処理した後、前処理を行った。冷延鋼板は、前処理としてアルカリ脱脂処理した後、フッ化水素酸（３０～５０％）／過酸化水素の液量比率が１／３０となるように混合し、液温度が１０℃になるよう調整し、鋼板を５秒浸漬し、その後、飽和の炭酸水素ナトリウムに浸漬して表面を中和し、水洗乾燥した。各めっき鋼板はアルカリ脱脂後に前処理として電気めっきにてＺｎめっきを施した。 In forming the film, the cold-rolled steel sheet or the plated steel sheet was subjected to alkaline degreasing treatment and then pretreatment. The cold-rolled steel sheet is subjected to alkaline degreasing treatment as a pretreatment, and then mixed so that the liquid amount ratio of hydrofluoric acid (30 to 50%) / hydrogen peroxide becomes 1/30, and the liquid temperature becomes 10 ° C. The steel sheet was soaked for 5 seconds, then soaked in saturated sodium hydrogen peroxide to neutralize the surface, washed with water and dried. Each plated steel sheet was Zn-plated by electroplating as a pretreatment after alkaline degreasing.
各皮膜は以下の方法により鋼板表面上に設けた。 Each film was provided on the surface of the steel sheet by the following method.
有機系皮膜のエポキシ系樹脂は、アミン変性エポキシ樹脂／ブロックイソシアネート硬化剤をロールコータにより鋼板表面に塗布し、１４０℃で焼付した。なお、膜厚については、ロールコータの速度を変えて適宜制御した。 For the epoxy resin of the organic film, an amine-modified epoxy resin / blocked isocyanate curing agent was applied to the surface of the steel sheet with a roll coater and baked at 140 ° C. The film thickness was appropriately controlled by changing the speed of the roll coater.
有機無機複合皮膜のエポキシ系樹脂／結晶性層状物は、あらかじめ硝酸マグネシウム・６水和物水溶液１１３ｇ／Ｌと硝酸アルミニウム・９水和物水溶液８３ｇ／Ｌに炭酸水素ナトリウム・１０水和物水溶液３１ｇ／Ｌを滴下することで精製し得られた沈殿物をろ過し、乾燥して得た結晶性層状物の［Ｍｇ０．６６７Ａｌ０．３３３（ＯＨ）２］［ＣＯ３ ２］０．１６７・０．５Ｈ２Ｏをアミン変性エポキシ樹脂／ブロックイソシアネート硬化剤と１０：２（アミン変性エポキシ樹脂／ブロックイソシアネート硬化剤：結晶性層状物）の質量比で混ぜ、ロールコータにより供試材に塗布し、１４０℃で焼付した。結晶性層状物が［Ｍｇ０．６６７Ａｌ０．３３３（ＯＨ）２］［ＣＯ３ ２］０．１６７・０．５Ｈ２ＯであることはＸＲＤ解析で確認した。なお、膜厚については、ロールコータの速度を変えて適宜制御した。 The epoxy resin / crystalline layered product of the organic-inorganic composite film is prepared in advance with magnesium nitrate / hexahydrate aqueous solution 113 g / L, aluminum nitrate / nine hydrate aqueous solution 83 g / L, and sodium hydrogen carbonate / tetrahydrate aqueous solution 31 g. The precipitate obtained by purifying by dropping / L was filtered and dried to obtain a crystalline layered product [Mg 0.667 Al 0.333 ( OH) 2 ] [CO 32 ] 0.167 . -Mix 0.5H 2 O with an amine-modified epoxy resin / blocked isocyanate curing agent in a mass ratio of 10: 2 (amine-modified epoxy resin / blocked isocyanate curing agent: crystalline layered material) and apply to the test material with a roll coater. And baked at 140 ° C. It was confirmed by XRD analysis that the crystalline layered product was [Mg 0.667 Al 0.333 (OH) 2 ] [CO 32 ] 0.167・0.5H 2 O. The film thickness was appropriately controlled by changing the speed of the roll coater.
無機系皮膜の塩基性硫酸亜鉛３～５水和物は、濃度：２０ｇ／Ｌ、温度：５０℃の硫酸亜鉛・７水和物水溶液に鋼板を浸漬し（浸漬時間については、皮膜Ｋ：３秒、皮膜Ｌ：６０秒、皮膜Ｍ：１００秒）、その後十分に水洗を行った後に乾燥して得た。塩基性硫酸亜鉛３～５水和物であることはＸＲＤ解析で確認した。なお、膜厚については、浸漬時間を変えて適宜制御した。 For the basic zinc sulfate 3-5 hydrate of the inorganic film, the steel sheet is immersed in a zinc sulfate heptahydrate aqueous solution having a concentration of 20 g / L and a temperature of 50 ° C. Seconds, film L: 60 seconds, film M: 100 seconds), followed by thorough washing with water and then drying. It was confirmed by XRD analysis that it was a basic zinc sulfate 3-5 hydrate. The film thickness was appropriately controlled by changing the immersion time.
このようにして得られた各鋼板について、皮膜の膜厚を測定した。有機系皮膜（エポキシ系樹脂）、有機無機複合皮膜（エポキシ系樹脂／結晶性層状物）は、ＦＩＢを用いて皮膜の断面を４５°にスパッタリングし、極低加速ＳＥＭで断面を観察し、任意の１０点を測定した平均値とした。無機系皮膜（塩基性硫酸亜鉛３～５水和物）は、蛍光Ｘ線分析装置で得られた値を膜厚とした。蛍光Ｘ線分析装置の測定条件として、管球の電圧および電流は３０ｋＶおよび１００ｍＡとし、分光結晶ＴＡＰに設定してＯ－Ｋα線の測定に際しては、そのピーク位置に加えてバックグラウンド位置での強度も測定し、Ｏ－Ｋα線の正味の強度が算出できるようにした。なお、ピーク位置およびバックグラウンド位置での積分時間は、それぞれ２０秒とした。また、試料ステージには、９６ｎｍ、５４ｎｍ、２４ｎｍの酸化シリコン皮膜を形成したシリコンウエハーをセットし、これら酸化シリコン皮膜のＯ－Ｋα線の強度を算出できるようにし、酸化膜厚とＯ－Ｋα線強度との検量線を作成し、酸化シリコン皮膜換算での値を膜厚とした。
The film thickness of each steel sheet thus obtained was measured. For the organic film (epoxy resin) and organic-inorganic composite film (epoxy resin / crystalline layered material), the cross section of the film is sputtered to 45 ° using FIB, and the cross section is observed with an extremely low acceleration SEM, which is optional. The 10 points of the above were measured and used as the average value. The film thickness of the inorganic film (
また、各非金属からなる皮膜を有する鋼板の摩擦係数を以下のようにして測定した。図１は摩擦係数測定装置を示す概略正面図である。同図に示すように、鋼板から採取した摩擦係数測定用試料１が試料台２に固定され、試料台２は、水平移動可能なスライドテーブル３の上面に固定されている。スライドテーブル３の下面には、これに接したローラ４を有する上下動可能なスライドテーブル支持台５が設けられ、これを押し上げることによりビード６による摩擦係数測定用試料１への押し付け荷重Ｎを測定するための第１ロードセル７がスライドテーブル支持台５に取り付けられている。上記押し付け力を作用させた状態でスライドテーブル３を水平方向へ移動させた際の摺動抵抗力Ｆを測定するために第２ロードセル８がレール９の上を動くように、スライドテーブル３の一方の端部に取り付けられている。なお、潤滑油としてスギムラ化学工業（株）製のプレス用洗浄油プレトンＲ３５２Ｌを摩擦係数測定用試料１の表面に塗布して試験を行った。図２は使用したビードの形状・寸法を示す概略斜視図である。ビード６の下面が試料１の表面に押し付けられた状態で摺動する。図２に示すビード６の形状は幅１０ｍｍ、試料の摺動方向長さ４ｍｍ、摺動方向両端の下部は曲率０．５ｍｍＲの曲面で構成され、試料が押し付けられるビード下面は幅１０ｍｍ、摺動方向長さ３ｍｍの平面を有する。摩擦係数測定試験は図２に示すビードを用い、押し付け荷重Ｎ：４００ｋｇｆ、試料の引き抜き速度（スライドテーブル３の水平移動速度）：１００ｃｍ／ｍｉｎとした。試料とビードとの間の摩擦係数μは、式：μ＝Ｆ／Ｎで算出した。
In addition, the coefficient of friction of the steel sheet having a film made of each non-metal was measured as follows. FIG. 1 is a schematic front view showing a friction coefficient measuring device. As shown in the figure, the
また、得られた鋼板について、クリアランス：５％、可動刃の速度：１ｍ／ｓｅｃとして、１００ｍｍ×３０ｍｍにせん断し、試験片を得た。得られた試験片のせん断端面の破断面がダイス側、せん断面がポンチ側になるようＲ＝１０ｍｍで１８０°曲げ加工を施した。曲げ加工後の試験片について、以下の評価を行った。 Further, the obtained steel sheet was sheared to 100 mm × 30 mm with a clearance of 5% and a speed of a movable blade of 1 m / sec to obtain a test piece. The obtained test piece was bent 180 ° at R = 10 mm so that the fracture surface of the sheared end surface was on the die side and the sheared surface was on the punch side. The following evaluations were made on the test pieces after bending.
（ひずみ抑制効果）
ひずみ抑制効果は、せん断時に刃と鋼板が接触する部分（図４参照。）における、金属光沢部（刃で鋼板表面が押しつぶされることによってできる平滑な面）の有無を観察した。金属光沢部が刃と鋼板の接触部分全体に存在する場合は抑制効果なし、金属光沢部がない場合は抑制効果ありと判断した。また、金属光沢部が点在する場合は、金属光沢部が一部ありと判断した。金属光沢部は、刃によって押しつぶされた箇所となり、鋼板に圧延加工を施して歪を与えた状態に類似する。このことから、金属光沢部がある場合はひずみ抑制効果なし、金属光沢部がない場合はひずみ抑制効果ありとした。
(Strain suppression effect)
As for the strain suppressing effect, the presence or absence of a metallic luster portion (a smooth surface formed by crushing the surface of the steel plate by the blade) was observed in the portion where the blade and the steel plate contact during shearing (see FIG. 4). It was judged that there was no suppressive effect when the metallic luster portion was present in the entire contact portion between the blade and the steel plate, and there was a suppressive effect when there was no metallic luster portion. When the metallic luster parts were scattered, it was judged that there were some metallic luster parts. The metallic luster portion becomes a portion crushed by a blade, which is similar to a state in which a steel plate is rolled and distorted. From this, it was determined that there was no strain suppressing effect when there was a metallic luster, and there was a strain suppressing effect when there was no metallic luster.
（微小き裂）
キーエンス製のマイクロスコープを用いて、図３に示す曲げＲ止まり部（曲げＲ加工を受けた部分）の曲げ部外側に発生したき裂の個数を確認した。き裂の個数が５個以下であれば抑制効果ありと判断した。
(Small crack)
Using a KEYENCE microscope, the number of cracks generated on the outside of the bent portion of the bent R stop portion (the portion subjected to the bending R processing) shown in FIG. 3 was confirmed. If the number of cracks was 5 or less, it was judged to have an inhibitory effect.
（遅れ破壊特性）
曲げ加工後、ボルト締結により曲げに伴うスプリングバック分を締め込み、曲げ頂点部の表層に応力を負荷した。曲げ加工およびボルト締結後の試験片の模式図を図３に示す。図３に示したボルト締め込み後の試験片をｐＨ３の塩酸に浸漬し、割れ発生までの時間で評価した。最大浸漬時間は１００時間とした。浸漬１００時間たっても割れなかったものは評価ａ、浸漬５０時間以上１００時間未満で割れたものは評価ｂ、浸漬１０時間以上５０時間未満で割れたものは評価ｃ、浸漬時間１０時間未満で割れたものは評価ｄとした。さらに１００時間で割れなかった評価aの材料を、追加でｐＨ２の塩酸に浸漬し、１００時間浸漬しても割れなかったものを評価ａ+とし、１００時間未満で割れたものは評価aのままとした。評価ａ+、ａまたはｂを合格と判断した。
(Delayed fracture characteristics)
After bending, the springback due to bending was tightened by bolting, and stress was applied to the surface layer of the bending apex. FIG. 3 shows a schematic diagram of the test piece after bending and bolting. The test piece after bolt tightening shown in FIG. 3 was immersed in hydrochloric acid having a pH of 3, and evaluated by the time until cracking occurred. The maximum immersion time was 100 hours. Evaluation a for those that did not crack even after 100 hours of immersion, evaluation b for those that cracked after 50 hours or more and less than 100 hours of immersion, evaluation c for those that cracked after 10 hours or more and less than 50 hours of immersion, cracking in less than 10 hours of immersion The one was evaluated as d. Further, the material of evaluation a that did not crack in 100 hours was additionally immersed in hydrochloric acid of
以上より得られた結果を表２に示す。 The results obtained from the above are shown in Table 2.
表２より、本発明はいずれも遅れ破壊特性に優れていることがわかる。 From Table 2, it can be seen that all of the present inventions are excellent in delayed fracture characteristics.
１ 摩擦係数測定用試料
２ 試料台
３ スライドテーブル
４ ローラ
５ スライドテーブル支持台
６ ビード
７ 第１ロードセル
８ 第２ロードセル
９ レール
Ｎ 押付荷重
Ｆ 摺動抵抗力
1 Sample for coefficient of
Claims (3)
（１／μ）×ｔ≧１００・・・（１）
なお、式（１）において、
μ：非金属からなる皮膜を有する鋼板の摩擦係数、ｔ：非金属からなる皮膜の膜厚（ｎｍ）
である。 A steel sheet having a tensile strength of 1180 MPa or more and having a film made of a non-metal on the surface of the steel sheet has a friction coefficient of 0.5 or less, the film thickness is 10 nm or more, and the non-metal film is further formed. A steel sheet in which the friction coefficient of a steel sheet having a film made of metal and the film thickness of the film satisfy the formula (1).
(1 / μ) × t ≧ 100 ... (1)
In addition, in equation (1)
μ: Friction coefficient of steel sheet having a film made of non-metal, t: Thickness of film made of non-metal (nm)
Is.
（１／μ）×ｔ≧１０００・・・（２）
なお、式（２）において、
μ：非金属からなる皮膜を有する鋼板の摩擦係数、ｔ：非金属からなる皮膜の膜厚（ｎｍ）
である。 The steel sheet according to claim 1 or 2, wherein the friction coefficient of the steel sheet having a film made of the non-metal and the film thickness of the film satisfy the formula (2).
(1 / μ) × t ≧ 1000 ... (2)
In addition, in equation (2)
μ: Friction coefficient of steel sheet having a film made of non-metal, t: Thickness of film made of non-metal (nm)
Is.
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